WO2018003167A1 - Method for producing silicon monocrystal - Google Patents
Method for producing silicon monocrystal Download PDFInfo
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- WO2018003167A1 WO2018003167A1 PCT/JP2017/006782 JP2017006782W WO2018003167A1 WO 2018003167 A1 WO2018003167 A1 WO 2018003167A1 JP 2017006782 W JP2017006782 W JP 2017006782W WO 2018003167 A1 WO2018003167 A1 WO 2018003167A1
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- single crystal
- oxygen concentration
- magnetic field
- limit value
- wafer
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/30—Mechanisms for rotating or moving either the melt or the crystal
- C30B15/305—Stirring of the melt
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Definitions
- the present invention relates to a method for producing a silicon single crystal.
- HMCZ method In the horizontal magnetic field application Czochralski method (HMCZ method), convection is likely to occur at the surface of the melt in the crucible and convection is suppressed at the bottom of the crucible, so that the oxygen concentration distribution in the crystal growth axis direction is made uniform. It has been proposed (Patent Document 1).
- the oxygen concentration in the range within about 10 mm from the outer peripheral edge of the wafer (hereinafter also referred to as the outer peripheral portion) is lower than the other central portions. Since such an outer peripheral portion can cause defects in the device process, in order to increase the device yield, it is required to make the oxygen concentration uniform up to the outer peripheral portion.
- the problem to be solved by the present invention is to provide a method for producing a silicon single crystal capable of making the oxygen concentration in the wafer surface uniform up to the outer peripheral portion while minimizing the production cost of the silicon single crystal. .
- the correlation between the diameter of the single crystal to be pulled up, the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer is obtained in advance for predetermined manufacturing conditions.
- the diameter of the single crystal to be pulled is determined from the correlation between the distribution characteristics of the oxygen concentration at the outer periphery of the wafer, the limit value of the horizontal magnetic field strength and the limit value of the crystal rotation of the single crystal, and the correlation.
- the correlation between the diameter of the pulled single crystal, the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration in the outer periphery of the wafer is obtained in advance for predetermined manufacturing conditions.
- the horizontal magnetic field strength to be applied is determined from the distribution characteristics of the allowable oxygen concentration at the outer periphery of the wafer, the limit value of the diameter of the single crystal to be pulled up, the limit value of the crystal rotation of the single crystal, and the above correlation.
- the correlation between the diameter of the pulled single crystal, the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration in the outer periphery of the wafer is obtained in advance for a predetermined manufacturing condition.
- the crystal rotation of the single crystal is obtained from the distribution characteristics of the oxygen concentration in the permissible outer periphery of the wafer, the limit value of the single crystal to be pulled up, the limit value of the horizontal magnetic field strength, and the correlation, and the calculation is performed.
- the correlation obtained by adding the diameter of the single crystal to be pulled to the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer in advance is obtained.
- the minimum value of the single crystal to be pulled is determined from the correlation between the limit value of the oxygen concentration distribution characteristic at the outer periphery of the wafer, the limit value of the horizontal magnetic field strength, the limit value of the crystal rotation of the single crystal, and the correlation. Find the diameter.
- the diameter of the single crystal to be pulled is minimized, so that the production cost of the silicon single crystal can be minimized.
- the distribution characteristic of the oxygen concentration at the outer peripheral portion of the wafer maintains the limit value, the oxygen concentration in the wafer surface can be made uniform.
- the correlation obtained by adding the diameter of the single crystal to be pulled to the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration in the outer periphery of the wafer in advance is obtained.
- the application is based on the correlation between the limit value of the oxygen concentration distribution characteristic at the outer periphery of the wafer, the limit value of the diameter of the single crystal to be pulled up, the limit value of the crystal rotation of the single crystal, and the correlation. Find the horizontal magnetic field strength to be used. As a result, the diameter of the single crystal to be pulled is minimized, so that the production cost of the silicon single crystal can be minimized. Further, since the distribution characteristic of the oxygen concentration at the outer peripheral portion of the wafer maintains the limit value, the oxygen concentration in the wafer surface can be made uniform.
- the correlation obtained by adding the diameter of the single crystal to be pulled to the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer in advance is obtained.
- the relationship between the limit value of the distribution characteristics of oxygen concentration at the outer periphery of the wafer, the limit value of the diameter of the single crystal to be pulled up, the limit value of the horizontal magnetic field strength, and the correlation Obtain crystal rotation.
- the diameter of the single crystal to be pulled is minimized, so that the production cost of the silicon single crystal can be minimized.
- the distribution characteristic of the oxygen concentration at the outer peripheral portion of the wafer maintains the limit value, the oxygen concentration in the wafer surface can be made uniform.
- 2 is a graph illustrating an example of a relationship between crystal rotation of a single crystal of the manufacturing apparatus illustrated in FIG. 1 and oxygen concentration distribution characteristics in a wafer outer peripheral portion. It is a graph which shows an example of the relationship between the position of the diameter direction of the wafer of the silicon single crystal manufactured with the manufacturing apparatus shown in FIG. 1, and oxygen concentration. 2 is a graph showing an example of the relationship between the diameter of a single crystal pulled by the manufacturing apparatus shown in FIG. 1 and the distribution characteristics of oxygen concentration in the outer periphery of the wafer.
- FIG. 1 is a cross-sectional view showing an example of a manufacturing apparatus to which a silicon single crystal manufacturing method according to an embodiment of the present invention is applied.
- a silicon single crystal manufacturing apparatus 1 (hereinafter also simply referred to as manufacturing apparatus 1) to which the manufacturing method of the present embodiment is applied includes a cylindrical first chamber 11 and a cylindrical second chamber 12, These are airtightly connected.
- a quartz crucible 21 containing the silicon melt M and a graphite crucible 22 protecting the quartz crucible 21 are supported by a support shaft 23 and driven.
- the mechanism 24 can be rotated and lifted.
- an annular heater 25 and an annular heat insulating cylinder 26 made of a heat insulating material are disposed so as to surround the quartz crucible 21 and the graphite crucible 22.
- a heater may be added below the crucible 21.
- a cylindrical heat shielding member 27 is provided inside the first chamber 11 and above the quartz crucible 21.
- the heat shielding member 27 is made of a counter metal such as molybdenum or tungsten or carbon, blocks radiation from the silicon melt M to the silicon single crystal C, and rectifies the gas flowing in the first chamber 11.
- the heat shielding member 27 is fixed to the heat retaining cylinder 26 using a bracket 28.
- a heat shield part is provided at the lower end of the heat shield member 27 so as to face the entire surface of the silicon melt M, so that radiation from the surface of the silicon melt M is cut and the surface of the silicon melt M is kept warm. May be.
- the second chamber 12 connected to the upper part of the first chamber 11 is a chamber for accommodating the grown silicon single crystal C and taking it out.
- a pulling mechanism 32 for pulling up the silicon single crystal while rotating it with the wire 31 is provided in the upper part of the second chamber 12.
- a seed crystal S is mounted on the chuck at the lower end of the wire 31 suspended from the pulling mechanism 32.
- An inert gas such as argon gas is introduced from a gas inlet 13 provided in the upper portion of the first chamber 11. This inert gas passes between the silicon single crystal C being pulled and the heat shielding member 27, then passes between the lower end of the heat shielding member 27 and the melt surface of the silicon melt M, and further quartz. After rising to the upper end of the made crucible 21, it is discharged from the gas discharge port 14.
- a magnetic field generator 41 that applies a magnetic field to the melt M in the quartz crucible 21 is disposed outside the first chamber 11 (made of a nonmagnetic shield material) so as to surround the first chamber 11.
- the magnetic field generator 41 generates a horizontal magnetic field toward the quartz crucible 21 and is constituted by an electromagnetic coil.
- the magnetic field generator 41 controls the thermal convection generated in the melt M in the quartz crucible 21, thereby stabilizing the crystal growth and suppressing micro variations in the impurity distribution in the crystal growth direction. In particular, when producing a large-diameter silicon single crystal, the effect is great.
- the magnetic field strength shown below is a value measured at the center position of the surface of the melt M in the quartz crucible 21.
- a quartz crucible 21 is filled with polycrystalline silicon and a silicon raw material to which a dopant is added if necessary. Then, the heater 25 is turned on and the silicon raw material is melted in the quartz crucible 21 to obtain a silicon melt M. Subsequently, the magnetic field generator 41 is turned on and the application of the horizontal magnetic field to the quartz crucible 21 is started, and the temperature of the silicon melt M is raised to the starting temperature.
- the quartz crucible 21 is rotated at a predetermined speed by the drive mechanism 24 while introducing an inert gas from the gas inlet 13 and discharging from the gas outlet 14, and the wire
- the seed crystal S attached to 31 is immersed in the silicon melt M.
- the wire 31 is also gently pulled up while rotating at a predetermined speed to form a seed stop, and then the diameter is increased to a desired diameter, and a silicon single crystal C having a substantially cylindrical straight body is grown.
- the liquid level of the silicon melt M in the quartz crucible 21 falls, and the conditions of the hot zone change including the application of a horizontal magnetic field from the magnetic field generator 41 to the quartz crucible 21. .
- the vertical height of the liquid level of the silicon melt M during the pulling of the silicon single crystal C is controlled by the drive mechanism 24 to be constant.
- the drive mechanism 24 is controlled, for example, by the position of the crucible 21, the position of the silicon melt M measured by a CCD camera or the like, the pulling length of the silicon single crystal C, the temperature in the first chamber 11, the silicon melt This is executed according to information such as the surface temperature of the liquid M, the flow rate of the inert gas, and the like, whereby the vertical position of the quartz crucible 21 is moved by the drive mechanism 24.
- FIG. 4 is a graph showing an example of distribution characteristics of oxygen concentration in the wafer state of the silicon single crystal C thus manufactured.
- the horizontal axis indicates the position in the diameter direction where the wafer center is 0, and the vertical axis indicates the oxygen concentration ( ⁇ 10 17 atoms / cm 3 ).
- the oxygen concentration referred to in this specification is a value measured by the FT-IR method (Fourier transform infrared spectrophotometry) standardized by ASTM F-121 (1979).
- the wafer outer peripheral portion referred to in this specification is a region from the outer peripheral end portion of the wafer to the inside of 10 mm.
- a drop in the oxygen concentration at the outer peripheral portion of the wafer an example of 5 mm from the outer peripheral end portion is shown in FIGS. 2, 3, and 5.
- the position is not limited to 5 mm.
- the oxygen concentration in the outer peripheral portion of the wafer is lower by about 0.5 ⁇ 10 17 atoms / cm 3 than other parts.
- a horizontal magnetic field is applied to control the thermal convection generated in the silicon melt M in the quartz crucible 21, thereby improving the pull-up diameter controllability. This is because the melt of the surface layer in which oxygen is evaporated is taken into the outer periphery of the crystal and the oxygen concentration in the outer periphery of the crystal is likely to decrease.
- the horizontal magnetic field strength by the magnetic field generator 41 is lowered, the decrease in oxygen concentration at the outer periphery of the wafer can be suppressed.
- the horizontal magnetic field strength by the magnetic field generator 41 is lowered, the controllability of the heat convection generated in the silicon melt M in the quartz crucible 21 is lowered, so that the pulling rate controllability is lowered.
- the horizontal magnetic field strength by the magnetic field generator 41 is lowered, the controllability of the heat convection generated in the silicon melt M in the quartz crucible 21 is lowered, so that the oxygen concentration is raised. Therefore, there is a certain limit value for reducing the horizontal magnetic field strength.
- the crystal rotation speed of the silicon single crystal C at the time of pulling up refers to the rotation speed of the silicon single crystal C using only the wire 31 and not the relative rotation speed considering the rotation speed of the quartz crucible 21. If it does so, the fall of the oxygen concentration in the outer peripheral part of a wafer can be suppressed. However, when the crystal rotation speed of the silicon single crystal C at the time of pulling is increased, the silicon single crystal C is twisted. Further, when the crystal rotation speed of the silicon single crystal C at the time of pulling is increased, the oxygen concentration increases. Therefore, there is a certain limit value for increasing the crystal rotation speed of the silicon single crystal C when it is pulled up.
- the diameter of the silicon single crystal C to be pulled up is set to a minimum value in consideration of the diameter variation due to the control variation such as the pulling speed. However, if this diameter is increased, the amount to be discarded increases. Manufacturing yield decreases. There is also a restriction on the size of the quartz crucible 21 of the manufacturing apparatus 1. Therefore, there is a certain limit value for increasing the diameter of the silicon single crystal C when it is pulled up.
- the present inventors have determined the correlation between how the horizontal magnetic field strength, the crystal rotation speed and the diameter of the silicon single crystal C each affect the oxygen concentration distribution characteristics of the outer periphery of the crystal. Verified.
- FIG. 2 shows an example of the relationship between the horizontal magnetic field strength and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer when the silicon single crystal C is manufactured under predetermined conditions using the predetermined manufacturing apparatus 1 shown in FIG. It is a graph to show.
- the horizontal axis indicates the horizontal magnetic field strength (Gauss, G, the right side is large and the left side is small) by the magnetic field generator 41, and the vertical axis is a position (hereinafter referred to as 5 mm) from the outer peripheral edge of the wafer toward the center.
- FIG. 3 shows the crystal rotation speed of the single crystal (referred to the rotation speed of the single crystal C itself) and the outer periphery of the wafer when the silicon single crystal C is manufactured using the manufacturing apparatus 1 shown in FIG. It is a graph of an example of the relationship with the distribution characteristic of oxygen concentration in.
- the horizontal axis represents the crystal rotation speed of the single crystal (rpm, the right side is large and the left side is small), and the vertical axis is the difference in oxygen concentration (Oi [In10] ⁇ Oi [In5], 10 17 atoms / cm 3 ). As described above, it can be seen that the oxygen concentration difference approaches zero when the crystal rotation speed is increased.
- FIG. 4 is a graph showing an example of oxygen concentration distribution characteristics in the wafer state of the silicon single crystal C when a 300 mm wafer is manufactured as described above.
- FIG. 5 uses the results shown in FIG. 4 and assumes that the distribution characteristics (oxygen behavior) of the oxygen concentration at the outer periphery of the pulled diameter do not change regardless of the diameter. This is a guessed graph.
- the horizontal axis shows the diameter of the single crystal set when pulling up (mm, the right side is large and the left side is small), and the vertical axis is the difference in oxygen concentration (Oi [In10]) as in FIGS. -Oi [In5], 10 17 atoms / cm 3 ).
- Oi [In10] the difference in oxygen concentration
- the oxygen concentration distribution characteristics (Oi [In10] ⁇ Oi [In5], 10 17 atoms / cm 3 ) at the outer periphery of the crystal are obtained from the horizontal magnetic field strength and the rotational speed of the silicon single crystal C.
- the diameter of the single crystal when pulled up is D (mm)
- the strength of the horizontal magnetic field is G (Gauss)
- the correlation was defined by the following formula.
- the constants a, b, c, and d correspond to weights for the horizontal magnetic field strength, the rotational speed and the diameter of the silicon single crystal, respectively.
- the limit value (allowable value) of the oxygen concentration distribution characteristic ⁇ at the outer peripheral portion of the wafer is the maximum value of the distribution value (sag value) of the outer peripheral oxygen concentration allowed for the wafer as a product.
- the product shipment standard set according to the above.
- Oi [In10] ⁇ Oi [In5] 0.5 ⁇ 10 17 atoms / cm 3 .
- the limit value of the horizontal magnetic field strength is a lower limit value in consideration of the controllability of the pulling rate and the increase in oxygen concentration as described above, and the manufacturing conditions for each silicon single crystal manufacturing apparatus 1 based on experience values and simulations. It is determined every time. For example, it is 2000G, 3000G or 4000G.
- the limit value of the crystal rotation speed of the single crystal at the time of pulling is an upper limit value in consideration of an increase in the bend and oxygen concentration, and is determined for each manufacturing condition for each manufacturing apparatus 1 based on experience values and simulations. For example, 8 rpm, 9 rpm, 10 rpm, 12 rpm, or 15 rpm.
- the limit value (allowable value) of the distribution characteristic ⁇ of the oxygen concentration at the outer periphery of the wafer is 0.1 ⁇ 10 17 atoms / cm 3
- the limit value of the horizontal magnetic field strength is 2500 G
- a single crystal crystal when pulling up When the limit value of the rotation speed is set to 8 rpm and is substituted into the above equation 2, the diameter D of the silicon single crystal obtained by this is 330 mm. If a silicon single crystal is manufactured with this diameter D as a set value, the distribution characteristic ⁇ of the oxygen concentration at the outer periphery of the wafer is satisfied to be 0.5 ⁇ 10 17 atoms / cm 3 or less, and the controllability of the pulling rate is high. It is possible to obtain an ingot that is good, suppresses an increase in oxygen concentration and bends, and further minimizes the amount of the outer peripheral portion discarded when processing into a wafer having a specified diameter.
- the limit value of the distribution characteristic ⁇ of the oxygen concentration at the outer periphery of the wafer, the limit value of the horizontal magnetic field strength, and the limit value of the crystal rotation speed of the single crystal at the time of pulling are substituted into Equation 2, thereby although the diameter D of the single crystal was obtained, instead of this, the limit value of the oxygen concentration distribution characteristic ⁇ at the outer periphery of the wafer, the limit value of the diameter of the silicon single crystal, and the crystal rotation of the single crystal at the time of pulling up
- a silicon single crystal may be manufactured by substituting the limit value of the velocity, thereby obtaining the horizontal magnetic field strength, and setting the obtained horizontal magnetic field strength.
- a single crystal of silicon may be manufactured by obtaining the crystal rotation speed of the first and setting the obtained crystal rotation speed.
- SYMBOLS 1 Manufacturing apparatus of a silicon single crystal 11 ... 1st chamber 12 ... 2nd chamber 13 ... Gas inlet 14 ... Gas outlet 21 ... Quartz crucible 22 ... Graphite crucible 23 ... Support shaft 24 ... Drive mechanism 25 ... Heater 26 ... Insulating cylinder 27 ... Heat shielding member 28 ... Bracket 31 ... Wire 32 ... Pulling mechanism 41 ... Magnetic field generator M ... Silicon melt C ... Silicon single crystal S ... Seed crystal
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Abstract
According to the present invention, correlations between a diameter (D) of a monocrystal (C) when being pulled up by a CZ process, a horizontal magnetic field strength (G) to be applied to a melt (M), a crystal rotation speed (V) of the monocrystal (C) being pulled up, and an oxygen concentration distribution characteristic (δ) at an outer periphery of a wafer are determined in advance for a prescribed production condition. Then, a minimum diameter of the monocrystal to be pulled up is determined on the basis of a limit value of the oxygen concentration distribution characteristic at the outer periphery of the wafer, a limit value of the horizontal magnetic field strength, a limit value of the crystal rotation speed of the monocrystal being pulled up, and the determined correlations. A silicon monocrystal is produced under the prescribed production condition using the determined minimum diameter as a target diameter.
Description
本発明は、シリコン単結晶の製造方法に関するものである。
The present invention relates to a method for producing a silicon single crystal.
水平磁場印加チョクラルスキー法(HMCZ法)において、坩堝内の融液の表面部では対流が起こり易くし、坩堝の底部では対流を抑制することにより、結晶成長軸方向の酸素濃度分布を均一にすることが提案されている(特許文献1)。
In the horizontal magnetic field application Czochralski method (HMCZ method), convection is likely to occur at the surface of the melt in the crucible and convection is suppressed at the bottom of the crucible, so that the oxygen concentration distribution in the crystal growth axis direction is made uniform. It has been proposed (Patent Document 1).
ところで、ウェーハの外周端部から10mm程度以内の範囲(以下、外周部ともいう)における酸素濃度は、その他の中央部分に比べて低い。こうした外周部はデバイスプロセスにおける不良を発生させる要因となり得ることから、デバイスの歩留まりを高くするために、外周部に至るまで酸素濃度の均一化が求められている。
By the way, the oxygen concentration in the range within about 10 mm from the outer peripheral edge of the wafer (hereinafter also referred to as the outer peripheral portion) is lower than the other central portions. Since such an outer peripheral portion can cause defects in the device process, in order to increase the device yield, it is required to make the oxygen concentration uniform up to the outer peripheral portion.
本発明が解決しようとする課題は、シリコン単結晶の製造コストを最小限に抑制しつつウェーハ面内の酸素濃度を外周部に至るまで均一にできるシリコン単結晶の製造方法を提供することである。
The problem to be solved by the present invention is to provide a method for producing a silicon single crystal capable of making the oxygen concentration in the wafer surface uniform up to the outer peripheral portion while minimizing the production cost of the silicon single crystal. .
第1の観点による発明は、引き上げられる単結晶の直径、水平磁場強度及び単結晶の結晶回転と、ウェーハ外周部における酸素濃度の分布特性との相関関係を、所定の製造条件について予め求めておき、許容されるウェーハ外周部における酸素濃度の分布特性、水平磁場強度の限界値及び単結晶の結晶回転の限界値と、前記相関関係とから、引き上げるべき単結晶の直径を求め、当該求められた直径の単結晶を前記所定の製造条件の下で製造することによって、上記課題を解決する。
In the invention according to the first aspect, the correlation between the diameter of the single crystal to be pulled up, the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer is obtained in advance for predetermined manufacturing conditions. The diameter of the single crystal to be pulled is determined from the correlation between the distribution characteristics of the oxygen concentration at the outer periphery of the wafer, the limit value of the horizontal magnetic field strength and the limit value of the crystal rotation of the single crystal, and the correlation. The above problem is solved by manufacturing a single crystal having a diameter under the predetermined manufacturing conditions.
第2の観点による発明は、引き上げられる単結晶の直径と、水平磁場強度と、単結晶の結晶回転と、ウェーハ外周部における酸素濃度の分布特性との相関関係を、所定の製造条件について予め求めておき、許容されるウェーハ外周部における酸素濃度の分布特性と、引き上げられる単結晶の直径の限界値と、単結晶の結晶回転の限界値と、前記相関関係とから、印加すべき水平磁場強度を求め、当該求められた水平磁場強度と前記所定の製造条件の下で単結晶を製造することによって、上記課題を解決する。
In the invention according to the second aspect, the correlation between the diameter of the pulled single crystal, the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration in the outer periphery of the wafer is obtained in advance for predetermined manufacturing conditions. The horizontal magnetic field strength to be applied is determined from the distribution characteristics of the allowable oxygen concentration at the outer periphery of the wafer, the limit value of the diameter of the single crystal to be pulled up, the limit value of the crystal rotation of the single crystal, and the above correlation. The above problem is solved by manufacturing a single crystal under the determined horizontal magnetic field strength and the predetermined manufacturing conditions.
第3の観点による発明は、引き上げられる単結晶の直径と、水平磁場強度と、単結晶の結晶回転と、ウェーハ外周部における酸素濃度の分布特性との相関関係を、所定の製造条件について予め求めておき、許容されるウェーハ外周部における酸素濃度の分布特性と、引き上げられる単結晶の限界値と、水平磁場強度の限界値と、前記相関関係とから、単結晶の結晶回転を求め、当該求められた結晶回転と前記所定の製造条件の下で単結晶を製造することによって、上記課題を解決する。
In the invention according to the third aspect, the correlation between the diameter of the pulled single crystal, the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration in the outer periphery of the wafer is obtained in advance for a predetermined manufacturing condition. The crystal rotation of the single crystal is obtained from the distribution characteristics of the oxygen concentration in the permissible outer periphery of the wafer, the limit value of the single crystal to be pulled up, the limit value of the horizontal magnetic field strength, and the correlation, and the calculation is performed. The above-mentioned problem is solved by manufacturing a single crystal under the specified crystal rotation and the predetermined manufacturing conditions.
特に限定はされないが、上記第1乃至第3の観点による発明において、前記相関関係は、引き上げられる単結晶の直径をD(mm)、水平磁場強度をG(ガウス)、単結晶の結晶回転をV(rpm)、ウェーハ外周部における酸素濃度の分布特性をδ(1017atoms/cm3)、a,b,c,dを定数としたときに、δ=aD+bG+cV+dなる式により定義し、予め前記定数a,b,c,dを求めておくことが望ましい。
Although not particularly limited, in the inventions according to the first to third aspects, the correlation is as follows: the diameter of the single crystal to be pulled is D (mm), the horizontal magnetic field strength is G (Gauss), and the crystal rotation of the single crystal is V (rpm), the distribution characteristics of the oxygen concentration at the outer periphery of the wafer are defined by the equation δ = aD + bG + cV + d, where δ (10 17 atoms / cm 3 ) and a, b, c, d are constants, It is desirable to obtain constants a, b, c, and d.
第1の観点による発明によれば、水平磁場強度と、単結晶の結晶回転と、ウェーハ外周部における酸素濃度の分布特性に、引き上げる単結晶の直径を加えた相関関係を予め求めておき、単結晶を製造する際においては、ウェーハ外周部における酸素濃度の分布特性の限界値と、水平磁場強度の限界値と、単結晶の結晶回転の限界値と、相関関係とから、引き上げる単結晶の最小の直径を求める。これにより、引き上げられる単結晶の直径が最小となるので、シリコン単結晶の生産コストを最小限に抑制することができる。また、ウェーハ外周部における酸素濃度の分布特性が限界値を維持するので、ウェーハ面内の酸素濃度を均一にすることができる。
According to the invention of the first aspect, the correlation obtained by adding the diameter of the single crystal to be pulled to the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer in advance is obtained. When manufacturing a crystal, the minimum value of the single crystal to be pulled is determined from the correlation between the limit value of the oxygen concentration distribution characteristic at the outer periphery of the wafer, the limit value of the horizontal magnetic field strength, the limit value of the crystal rotation of the single crystal, and the correlation. Find the diameter. As a result, the diameter of the single crystal to be pulled is minimized, so that the production cost of the silicon single crystal can be minimized. Further, since the distribution characteristic of the oxygen concentration at the outer peripheral portion of the wafer maintains the limit value, the oxygen concentration in the wafer surface can be made uniform.
第2の観点による発明によれば、水平磁場強度と、単結晶の結晶回転と、ウェーハ外周部における酸素濃度の分布特性に、引き上げられる単結晶の直径を加えた相関関係を予め求めておき、単結晶を製造する際においては、ウェーハ外周部における酸素濃度の分布特性の限界値と、引き上げられる単結晶の直径の限界値と、単結晶の結晶回転の限界値と、相関関係とから、印加すべき水平磁場強度を求める。これにより、引き上げられる単結晶の直径が最小となるので、シリコン単結晶の生産コストを最小限に抑制することができる。また、ウェーハ外周部における酸素濃度の分布特性が限界値を維持するので、ウェーハ面内の酸素濃度を均一にすることができる。
According to the invention according to the second aspect, the correlation obtained by adding the diameter of the single crystal to be pulled to the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration in the outer periphery of the wafer in advance is obtained. When manufacturing a single crystal, the application is based on the correlation between the limit value of the oxygen concentration distribution characteristic at the outer periphery of the wafer, the limit value of the diameter of the single crystal to be pulled up, the limit value of the crystal rotation of the single crystal, and the correlation. Find the horizontal magnetic field strength to be used. As a result, the diameter of the single crystal to be pulled is minimized, so that the production cost of the silicon single crystal can be minimized. Further, since the distribution characteristic of the oxygen concentration at the outer peripheral portion of the wafer maintains the limit value, the oxygen concentration in the wafer surface can be made uniform.
第3の観点による発明によれば、水平磁場強度と、単結晶の結晶回転と、ウェーハ外周部における酸素濃度の分布特性に、引き上げられる単結晶の直径を加えた相関関係を予め求めておき、単結晶を製造する際においては、ウェーハ外周部における酸素濃度の分布特性の限界値と、引き上げられる単結晶の直径の限界値と、水平磁場強度の限界値と、相関関係とから、単結晶の結晶回転を求める。これにより、引き上げられる単結晶の直径が最小となるので、シリコン単結晶の生産コストを最小限に抑制することができる。また、ウェーハ外周部における酸素濃度の分布特性が限界値を維持するので、ウェーハ面内の酸素濃度を均一にすることができる。
According to the invention of the third aspect, the correlation obtained by adding the diameter of the single crystal to be pulled to the horizontal magnetic field strength, the crystal rotation of the single crystal, and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer in advance is obtained. When manufacturing a single crystal, the relationship between the limit value of the distribution characteristics of oxygen concentration at the outer periphery of the wafer, the limit value of the diameter of the single crystal to be pulled up, the limit value of the horizontal magnetic field strength, and the correlation Obtain crystal rotation. As a result, the diameter of the single crystal to be pulled is minimized, so that the production cost of the silicon single crystal can be minimized. Further, since the distribution characteristic of the oxygen concentration at the outer peripheral portion of the wafer maintains the limit value, the oxygen concentration in the wafer surface can be made uniform.
以下、本発明の実施形態を図面に基づいて説明する。図1は、本発明の一実施の形態であるシリコン単結晶の製造方法が適用される製造装置の一例を示す断面図である。本実施形態の製造方法が適用されるシリコン単結晶の製造装置1(以下、単に製造装置1ともいう)は、円筒状の第1チャンバ11と、同じく円筒状の第2チャンバ12とを備え、これらは気密に接続されている。
Hereinafter, embodiments of the present invention will be described with reference to the drawings. FIG. 1 is a cross-sectional view showing an example of a manufacturing apparatus to which a silicon single crystal manufacturing method according to an embodiment of the present invention is applied. A silicon single crystal manufacturing apparatus 1 (hereinafter also simply referred to as manufacturing apparatus 1) to which the manufacturing method of the present embodiment is applied includes a cylindrical first chamber 11 and a cylindrical second chamber 12, These are airtightly connected.
第1チャンバ11の内部には、シリコン融液Mを収容する石英製の坩堝21と、この石英製の坩堝21を保護する黒鉛製の坩堝22とが、支持軸23で支持されるとともに、駆動機構24によって回転及び昇降が可能とされている。また、石英製の坩堝21と黒鉛製の坩堝22とを取り囲むように、環状のヒータ25と、同じく環状の、断熱材からなる保温筒26が配置されている。坩堝21の下方にヒータを追加してもよい。
Inside the first chamber 11, a quartz crucible 21 containing the silicon melt M and a graphite crucible 22 protecting the quartz crucible 21 are supported by a support shaft 23 and driven. The mechanism 24 can be rotated and lifted. Further, an annular heater 25 and an annular heat insulating cylinder 26 made of a heat insulating material are disposed so as to surround the quartz crucible 21 and the graphite crucible 22. A heater may be added below the crucible 21.
第1チャンバ11の内部であって、石英製の坩堝21の上部には、円筒状の熱遮蔽部材27が設けられている。熱遮蔽部材27は、モリブデン、タングステンなどの対価金属又はカーボンからなり、シリコン融液Mからシリコン単結晶Cへの放射を遮断するとともに、第1チャンバ11内を流れるガスを整流する。熱遮蔽部材27は、保温筒26にブラケット28を用いて固定されている。この熱遮蔽部材27の下端に、シリコン融液Mの全面と対向するように遮熱部を設け、シリコン融液Mの表面からの輻射をカットするとともにシリコン融液Mの表面を保温するようにしてもよい。
A cylindrical heat shielding member 27 is provided inside the first chamber 11 and above the quartz crucible 21. The heat shielding member 27 is made of a counter metal such as molybdenum or tungsten or carbon, blocks radiation from the silicon melt M to the silicon single crystal C, and rectifies the gas flowing in the first chamber 11. The heat shielding member 27 is fixed to the heat retaining cylinder 26 using a bracket 28. A heat shield part is provided at the lower end of the heat shield member 27 so as to face the entire surface of the silicon melt M, so that radiation from the surface of the silicon melt M is cut and the surface of the silicon melt M is kept warm. May be.
第1チャンバ11の上部に接続された第2チャンバ12は、育成したシリコン単結晶Cを収容し、これを取り出すためのチャンバである。第2チャンバ12の上部には、シリコン単結晶をワイヤ31で回転させながら引上げる引上げ機構32が設けられている。引上げ機構32から垂下されたワイヤ31の下端のチャックには種結晶Sが装着される。第1チャンバ11の上部に設けられたガス導入口13から、アルゴンガス等の不活性ガスが導入される。この不活性ガスは、引上げ中のシリコン単結晶Cと熱遮蔽部材27との間を通過した後、熱遮蔽部材27の下端とシリコン融液Mの融液面との間を通過し、さらに石英製の坩堝21の上端へ立ち上がった後、ガス排出口14から排出される。
The second chamber 12 connected to the upper part of the first chamber 11 is a chamber for accommodating the grown silicon single crystal C and taking it out. A pulling mechanism 32 for pulling up the silicon single crystal while rotating it with the wire 31 is provided in the upper part of the second chamber 12. A seed crystal S is mounted on the chuck at the lower end of the wire 31 suspended from the pulling mechanism 32. An inert gas such as argon gas is introduced from a gas inlet 13 provided in the upper portion of the first chamber 11. This inert gas passes between the silicon single crystal C being pulled and the heat shielding member 27, then passes between the lower end of the heat shielding member 27 and the melt surface of the silicon melt M, and further quartz. After rising to the upper end of the made crucible 21, it is discharged from the gas discharge port 14.
第1チャンバ11(非磁気シールド材からなる)の外側には、第1チャンバ11を取り囲むように、石英製の坩堝21内の融液Mに磁場を与える磁場発生装置41が配置されている。磁場発生装置41は、石英製の坩堝21に向けて、水平磁場を生じさせるものであり、電磁コイルで構成されている。磁場発生装置41は、石英製の坩堝21内の融液Mに生じた熱対流を制御することで、結晶成長を安定させ、結晶成長方向における不純物分布のミクロなバラツキを抑制する。特に大口径のシリコン単結晶を製造する場合にはその効果が大きい。なお、以下に示す磁場強度は、石英製の坩堝21内の融液Mの液面の中心位置で測定した値である。
A magnetic field generator 41 that applies a magnetic field to the melt M in the quartz crucible 21 is disposed outside the first chamber 11 (made of a nonmagnetic shield material) so as to surround the first chamber 11. The magnetic field generator 41 generates a horizontal magnetic field toward the quartz crucible 21 and is constituted by an electromagnetic coil. The magnetic field generator 41 controls the thermal convection generated in the melt M in the quartz crucible 21, thereby stabilizing the crystal growth and suppressing micro variations in the impurity distribution in the crystal growth direction. In particular, when producing a large-diameter silicon single crystal, the effect is great. The magnetic field strength shown below is a value measured at the center position of the surface of the melt M in the quartz crucible 21.
本実施形態の製造装置1を用いて、CZ法によりシリコン単結晶を育成するには、まず、石英製の坩堝21内に、多結晶シリコン及び必要に応じてドーパントを添加したシリコン原料を充填し、ヒータ25をONして石英製の坩堝21内でシリコン原料を融解し、シリコン融液Mとする。続いて、磁場発生装置41をONして石英製の坩堝21への水平磁場の印加を開始しつつ、シリコン融液Mの温度を引き上げ開始温度となるように調温する。シリコン融液Mの温度と磁場強度が安定したら、ガス導入口13から不活性ガスを導入しガス排出口14から排出しながら、駆動機構24によって石英製の坩堝21を所定速度で回転させ、ワイヤ31に装着された種結晶Sをシリコン融液Mに浸漬する。そして、ワイヤ31も所定速度で回転させながら静かに引上げて種絞りを形成した後、所望の直径まで拡径し、略円柱形状の直胴部を有するシリコン単結晶Cを成長させる。
In order to grow a silicon single crystal by the CZ method using the production apparatus 1 of the present embodiment, first, a quartz crucible 21 is filled with polycrystalline silicon and a silicon raw material to which a dopant is added if necessary. Then, the heater 25 is turned on and the silicon raw material is melted in the quartz crucible 21 to obtain a silicon melt M. Subsequently, the magnetic field generator 41 is turned on and the application of the horizontal magnetic field to the quartz crucible 21 is started, and the temperature of the silicon melt M is raised to the starting temperature. When the temperature and the magnetic field strength of the silicon melt M are stabilized, the quartz crucible 21 is rotated at a predetermined speed by the drive mechanism 24 while introducing an inert gas from the gas inlet 13 and discharging from the gas outlet 14, and the wire The seed crystal S attached to 31 is immersed in the silicon melt M. Then, the wire 31 is also gently pulled up while rotating at a predetermined speed to form a seed stop, and then the diameter is increased to a desired diameter, and a silicon single crystal C having a substantially cylindrical straight body is grown.
シリコン単結晶Cの引き上げにともない石英製の坩堝21のシリコン融液Mの液面が下がり、磁場発生装置41から石英製の坩堝21への水平磁場の印加を含めてホットゾーンの条件が変動する。この液面の変動を抑制するため、シリコン単結晶Cの引き上げ中におけるシリコン融液Mの液面の鉛直方向の高さは、駆動機構24によって一定となるように制御される。この駆動機構24の制御は、例えば、坩堝21の位置、CCDカメラなどで測定したシリコン融液Mの液面の位置、シリコン単結晶Cの引上げ長さ、第1チャンバ11内の温度、シリコン融液Mの表面温度、不活性ガス流量等の情報に応じて実行され、これにより石英製の坩堝21の上下方向の位置が駆動機構24によって移動する。
As the silicon single crystal C is pulled up, the liquid level of the silicon melt M in the quartz crucible 21 falls, and the conditions of the hot zone change including the application of a horizontal magnetic field from the magnetic field generator 41 to the quartz crucible 21. . In order to suppress this fluctuation of the liquid level, the vertical height of the liquid level of the silicon melt M during the pulling of the silicon single crystal C is controlled by the drive mechanism 24 to be constant. The drive mechanism 24 is controlled, for example, by the position of the crucible 21, the position of the silicon melt M measured by a CCD camera or the like, the pulling length of the silicon single crystal C, the temperature in the first chamber 11, the silicon melt This is executed according to information such as the surface temperature of the liquid M, the flow rate of the inert gas, and the like, whereby the vertical position of the quartz crucible 21 is moved by the drive mechanism 24.
さて、例えば300mmウェーハを製造する場合、シリコン単結晶Cの引上げ直径は、ばらつきを考慮して300mmより僅かに大きい所定値に設定される。図4は、そのようにして製造されたシリコン単結晶Cのウェーハ状態における酸素濃度の分布特性の一例を示すグラフである。横軸は、ウェーハ中心を0とする直径方向の位置を示し、縦軸は酸素濃度(×1017atoms/cm3)を示す。なお、本明細書にいう酸素濃度は、全てASTM F-121(1979)に規格されたFT-IR法(フーリエ変換赤外分光光度法)による測定値である。また本明細書にいうウェーハ外周部とは、ウェーハの外周端部から10mm内側までの領域である。以下の例では、ウェーハ外周部の酸素濃度の落込みとして、外周端部から5mmの事例を図2、3、5に示したが、これはウェーハ外周部の代表例として示したものであり、5mmの位置に限定するものではない。この例によると、ウェーハの外周部における酸素濃度は、他の部位に比べて0.5×1017atoms/cm3程度低くなっている。ウェーハの大径化にともなって水平磁場を印加し、石英製の坩堝21内のシリコン融液Mに生じた熱対流を制御することで引上げ直径の制御性を改善すると、熱対流による融液酸素の撹拌が行われ難く、酸素が蒸発した表層の融液が結晶外周部に取り込まれ、結晶外周部の酸素濃度が低下し易くなるからである。
For example, when manufacturing a 300 mm wafer, the pulling diameter of the silicon single crystal C is set to a predetermined value slightly larger than 300 mm in consideration of variation. FIG. 4 is a graph showing an example of distribution characteristics of oxygen concentration in the wafer state of the silicon single crystal C thus manufactured. The horizontal axis indicates the position in the diameter direction where the wafer center is 0, and the vertical axis indicates the oxygen concentration (× 10 17 atoms / cm 3 ). The oxygen concentration referred to in this specification is a value measured by the FT-IR method (Fourier transform infrared spectrophotometry) standardized by ASTM F-121 (1979). Further, the wafer outer peripheral portion referred to in this specification is a region from the outer peripheral end portion of the wafer to the inside of 10 mm. In the following example, as a drop in the oxygen concentration at the outer peripheral portion of the wafer, an example of 5 mm from the outer peripheral end portion is shown in FIGS. 2, 3, and 5. The position is not limited to 5 mm. According to this example, the oxygen concentration in the outer peripheral portion of the wafer is lower by about 0.5 × 10 17 atoms / cm 3 than other parts. As the diameter of the wafer is increased, a horizontal magnetic field is applied to control the thermal convection generated in the silicon melt M in the quartz crucible 21, thereby improving the pull-up diameter controllability. This is because the melt of the surface layer in which oxygen is evaporated is taken into the outer periphery of the crystal and the oxygen concentration in the outer periphery of the crystal is likely to decrease.
したがって、磁場発生装置41による水平磁場強度を下げれば、ウェーハの外周部における酸素濃度の低下は抑制できる。しかしながら、磁場発生装置41による水平磁場強度を下げると、石英製の坩堝21内のシリコン融液Mに生じた熱対流の制御性が低下するので、引上げ速度の制御性が低下する。また、磁場発生装置41による水平磁場強度を下げると、石英製の坩堝21内のシリコン融液Mに生じた熱対流の制御性が低下するので、酸素濃度が上昇する。したがって、水平磁場強度を下げることにも、一定の限界値がある。
Therefore, if the horizontal magnetic field strength by the magnetic field generator 41 is lowered, the decrease in oxygen concentration at the outer periphery of the wafer can be suppressed. However, when the horizontal magnetic field strength by the magnetic field generator 41 is lowered, the controllability of the heat convection generated in the silicon melt M in the quartz crucible 21 is lowered, so that the pulling rate controllability is lowered. Further, when the horizontal magnetic field strength by the magnetic field generator 41 is lowered, the controllability of the heat convection generated in the silicon melt M in the quartz crucible 21 is lowered, so that the oxygen concentration is raised. Therefore, there is a certain limit value for reducing the horizontal magnetic field strength.
また、引き上げる際のシリコン単結晶Cの結晶回転速度(ワイヤ31のみによるシリコン単結晶Cの回転速度をいい、石英製の坩堝21の回転速度を加味した相対的な回転速度ではない。)を大きくすれば、ウェーハの外周部における酸素濃度の低下は抑制できる。しかしながら、引き上げる際のシリコン単結晶Cの結晶回転速度を大きくすると、シリコン単結晶Cにくねりが発生する。また、引き上げる際のシリコン単結晶Cの結晶回転速度を大きくすると、酸素濃度が上昇する。したがって、引き上げる際のシリコン単結晶Cの結晶回転速度を大きくすることにも、一定の限界値がある。
In addition, the crystal rotation speed of the silicon single crystal C at the time of pulling up (refers to the rotation speed of the silicon single crystal C using only the wire 31 and not the relative rotation speed considering the rotation speed of the quartz crucible 21). If it does so, the fall of the oxygen concentration in the outer peripheral part of a wafer can be suppressed. However, when the crystal rotation speed of the silicon single crystal C at the time of pulling is increased, the silicon single crystal C is twisted. Further, when the crystal rotation speed of the silicon single crystal C at the time of pulling is increased, the oxygen concentration increases. Therefore, there is a certain limit value for increasing the crystal rotation speed of the silicon single crystal C when it is pulled up.
なお、引き上げるシリコン単結晶Cの直径は、引上げ速度などの制御ばらつきに起因する直径のばらつきを考慮した最小値が設定されているが、この直径を大きくすれば、廃棄される量が多くなって製造歩留まりが低下する。また、製造装置1の石英製の坩堝21などの大きさの制約もある。したがって、引き上げる際のシリコン単結晶Cの直径を大きくすることにも、一定の限界値がある。
The diameter of the silicon single crystal C to be pulled up is set to a minimum value in consideration of the diameter variation due to the control variation such as the pulling speed. However, if this diameter is increased, the amount to be discarded increases. Manufacturing yield decreases. There is also a restriction on the size of the quartz crucible 21 of the manufacturing apparatus 1. Therefore, there is a certain limit value for increasing the diameter of the silicon single crystal C when it is pulled up.
そこで、本発明者らは、水平磁場強度、シリコン単結晶Cの結晶回転速度及び直径のそれぞれが、結晶外周部の酸素濃度の分布特性に対してどのように影響しているか、その相関関係を検証した。
Therefore, the present inventors have determined the correlation between how the horizontal magnetic field strength, the crystal rotation speed and the diameter of the silicon single crystal C each affect the oxygen concentration distribution characteristics of the outer periphery of the crystal. Verified.
図2は、図1に示す所定の製造装置1を用いてシリコン単結晶Cを所定条件にて製造した場合における、水平磁場強度と、ウェーハ外周部における酸素濃度の分布特性との関係の一例を示すグラフである。横軸は、磁場発生装置41による水平磁場強度(ガウス,G,右側が大、左側が小を示す。)を示し、縦軸は、ウェーハの外周端から中心に向かって5mmの位置(以下、In5ともいう)と、同じくウェーハの外周端から中心に向かって100mmの位置(以下、In10ともいう)のそれぞれにおける酸素濃度の差(Oi[In10]-Oi[In5],1017atoms/cm3)を示す。上述したとおり、水平磁場強度を下げれば酸素濃度の差はゼロに近づくことが解る。
FIG. 2 shows an example of the relationship between the horizontal magnetic field strength and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer when the silicon single crystal C is manufactured under predetermined conditions using the predetermined manufacturing apparatus 1 shown in FIG. It is a graph to show. The horizontal axis indicates the horizontal magnetic field strength (Gauss, G, the right side is large and the left side is small) by the magnetic field generator 41, and the vertical axis is a position (hereinafter referred to as 5 mm) from the outer peripheral edge of the wafer toward the center. (Also referred to as In5) and a difference in oxygen concentration (Oi [In10] −Oi [In5], 10 17 atoms / cm 3 ) at 100 mm from the outer peripheral edge of the wafer toward the center (hereinafter also referred to as In10). ). As described above, it can be understood that if the horizontal magnetic field strength is lowered, the difference in oxygen concentration approaches zero.
図3は、図1に示す製造装置1を用いてシリコン単結晶Cを所定条件にて製造した場合における、単結晶の結晶回転速度(単結晶C自体の回転速度をいう)と、ウェーハ外周部における酸素濃度の分布特性との関係の一例をグラフである。横軸は、単結晶の結晶回転速度(rpm,右側が大、左側が小を示す。)を示し、縦軸は、図2と同じく酸素濃度の差(Oi[In10]-Oi[In5],1017atoms/cm3)を示す。上述したとおり、結晶回転速度を大きくすれば酸素濃度の差はゼロに近づくことが解る。
FIG. 3 shows the crystal rotation speed of the single crystal (referred to the rotation speed of the single crystal C itself) and the outer periphery of the wafer when the silicon single crystal C is manufactured using the manufacturing apparatus 1 shown in FIG. It is a graph of an example of the relationship with the distribution characteristic of oxygen concentration in. The horizontal axis represents the crystal rotation speed of the single crystal (rpm, the right side is large and the left side is small), and the vertical axis is the difference in oxygen concentration (Oi [In10] −Oi [In5], 10 17 atoms / cm 3 ). As described above, it can be seen that the oxygen concentration difference approaches zero when the crystal rotation speed is increased.
図4は、上述したとおり300mmウェーハを製造した場合の、シリコン単結晶Cのウェーハ状態における酸素濃度の分布特性の一例を示すグラフである。図5は、図4に示す結果を用い、引上げ直径の外周部の酸素濃度の分布特性(酸素挙動)は、直径によらず変化はないと仮定した上で、増径した時の酸素濃度を推測したグラフである。横軸は引き上げる際に設定される単結晶の直径(mm,右側が大、左側が小を示す。)を示し、縦軸は、図2及び図3と同じく酸素濃度の差(Oi[In10]-Oi[In5],1017atoms/cm3)を示す。上述したとおり、引き上げる際の単結晶の直径を大きく設定すれば酸素濃度の差はゼロに近づくことが解る。
FIG. 4 is a graph showing an example of oxygen concentration distribution characteristics in the wafer state of the silicon single crystal C when a 300 mm wafer is manufactured as described above. FIG. 5 uses the results shown in FIG. 4 and assumes that the distribution characteristics (oxygen behavior) of the oxygen concentration at the outer periphery of the pulled diameter do not change regardless of the diameter. This is a guessed graph. The horizontal axis shows the diameter of the single crystal set when pulling up (mm, the right side is large and the left side is small), and the vertical axis is the difference in oxygen concentration (Oi [In10]) as in FIGS. -Oi [In5], 10 17 atoms / cm 3 ). As described above, it can be seen that the difference in oxygen concentration approaches zero if the diameter of the single crystal when pulling is set large.
これら図2~図5の結果から、結晶外周部の酸素濃度の分布特性(Oi[In10]-Oi[In5],1017atoms/cm3)は、水平磁場強度、シリコン単結晶Cの回転速度及び直径のそれぞれと相関関係があることが解ったので、本発明者らは、引き上げる際の単結晶の直径をD(mm)、水平磁場強度をG(ガウス)、引き上げる際の単結晶の結晶回転速度をV(rpm)、ウェーハ外周部における酸素濃度の分布特性をδ(1017atoms/cm3)、a,b,c,dを定数としたときに、
[数1]
δ=aD+bG+cV+d…(式1)
なる式により相関関係を定義した。定数a,b,c,dは、水平磁場強度、シリコン単結晶の回転速度及び直径のそれぞれに対する重みに相当する。 2 to 5, the oxygen concentration distribution characteristics (Oi [In10] −Oi [In5], 10 17 atoms / cm 3 ) at the outer periphery of the crystal are obtained from the horizontal magnetic field strength and the rotational speed of the silicon single crystal C. And the diameter of the single crystal when pulled up is D (mm), the strength of the horizontal magnetic field is G (Gauss), and the crystal of the single crystal when pulled up When the rotational speed is V (rpm), the oxygen concentration distribution characteristic at the outer periphery of the wafer is δ (10 17 atoms / cm 3 ), and a, b, c, d are constants,
[Equation 1]
δ = aD + bG + cV + d (Formula 1)
The correlation was defined by the following formula. The constants a, b, c, and d correspond to weights for the horizontal magnetic field strength, the rotational speed and the diameter of the silicon single crystal, respectively.
[数1]
δ=aD+bG+cV+d…(式1)
なる式により相関関係を定義した。定数a,b,c,dは、水平磁場強度、シリコン単結晶の回転速度及び直径のそれぞれに対する重みに相当する。 2 to 5, the oxygen concentration distribution characteristics (Oi [In10] −Oi [In5], 10 17 atoms / cm 3 ) at the outer periphery of the crystal are obtained from the horizontal magnetic field strength and the rotational speed of the silicon single crystal C. And the diameter of the single crystal when pulled up is D (mm), the strength of the horizontal magnetic field is G (Gauss), and the crystal of the single crystal when pulled up When the rotational speed is V (rpm), the oxygen concentration distribution characteristic at the outer periphery of the wafer is δ (10 17 atoms / cm 3 ), and a, b, c, d are constants,
[Equation 1]
δ = aD + bG + cV + d (Formula 1)
The correlation was defined by the following formula. The constants a, b, c, and d correspond to weights for the horizontal magnetic field strength, the rotational speed and the diameter of the silicon single crystal, respectively.
そして、シリコン単結晶の製造装置1毎の所定の製造条件の下で予め定数a,b,c,dを求めておき、ウェーハ外周部における酸素濃度の分布特性δの限界値(許容値でもよい)と、水平磁場強度の限界値と、引き上げる際の単結晶の結晶回転速度の限界値とを上記式1に代入し、これにより求められるシリコン単結晶の直径D(=(δ-bG-cV-d)/a)を、引上げるシリコン単結晶Cの直径に設定する。
Then, constants a, b, c, and d are obtained in advance under predetermined manufacturing conditions for each silicon single crystal manufacturing apparatus 1, and the limit value (allowable value) of the oxygen concentration distribution characteristic δ at the outer periphery of the wafer is obtained. ), The limit value of the horizontal magnetic field strength, and the limit value of the crystal rotation speed of the single crystal at the time of pulling up are substituted into the above equation 1, and the silicon single crystal diameter D (= (δ−bG−cV) obtained by this is substituted. -D) / a) is set to the diameter of the silicon single crystal C to be pulled up.
ここで、ウェーハ外周部における酸素濃度の分布特性δの限界値(許容値)とは、製品としてのウェーハに許容される外周部の酸素濃度の分布値(落ち込み値)の最大値であり、デバイスなどに応じて設定される製品出荷基準などである。例えばOi[In10]-Oi[In5]=0.5×1017atoms/cm3である。また、水平磁場強度の限界値とは、上述したとおり引上げ速度の制御性や酸素濃度の増加を考慮した下限値であり、経験値やシミュレーションに基づいてシリコン単結晶の製造装置1毎の製造条件毎に定められる。例えば2000G,3000G又は4000Gである。また、引き上げる際の単結晶の結晶回転速度の限界値とは、くねりや酸素濃度の増加を考慮した上限値であり、経験値やシミュレーションに基づいて製造装置1毎の製造条件毎に定められる。例えば8rpm,9rpm,10rpm,12rpm又は15rpmである。
Here, the limit value (allowable value) of the oxygen concentration distribution characteristic δ at the outer peripheral portion of the wafer is the maximum value of the distribution value (sag value) of the outer peripheral oxygen concentration allowed for the wafer as a product. The product shipment standard set according to the above. For example, Oi [In10] −Oi [In5] = 0.5 × 10 17 atoms / cm 3 . Further, the limit value of the horizontal magnetic field strength is a lower limit value in consideration of the controllability of the pulling rate and the increase in oxygen concentration as described above, and the manufacturing conditions for each silicon single crystal manufacturing apparatus 1 based on experience values and simulations. It is determined every time. For example, it is 2000G, 3000G or 4000G. Moreover, the limit value of the crystal rotation speed of the single crystal at the time of pulling is an upper limit value in consideration of an increase in the bend and oxygen concentration, and is determined for each manufacturing condition for each manufacturing apparatus 1 based on experience values and simulations. For example, 8 rpm, 9 rpm, 10 rpm, 12 rpm, or 15 rpm.
図2~図5に示す実例を回帰分析することにより、式1の定数a,b,c,dの一例を求めたところ、下記のとおりであった。
[数2]
δ=-0.0166D+0.0005G-0.4836V+8.1984…(式2) An example of constants a, b, c, and d inEquation 1 was obtained by regression analysis of the examples shown in FIGS. 2 to 5 and was as follows.
[Equation 2]
δ = −0.0166D + 0.0005G−0.4836V + 8.11984 (Formula 2)
[数2]
δ=-0.0166D+0.0005G-0.4836V+8.1984…(式2) An example of constants a, b, c, and d in
[Equation 2]
δ = −0.0166D + 0.0005G−0.4836V + 8.11984 (Formula 2)
上記式2において、ウェーハ外周部における酸素濃度の分布特性δの限界値(許容値)を0.1×1017atoms/cm3、水平磁場強度の限界値を2500G、引き上げる際の単結晶の結晶回転速度の限界値を8rpmとして上記式2に代入すると、これにより求められるシリコン単結晶の直径Dは、330mmとなる。この直径Dを設定値としてシリコン単結晶を製造すれば、ウェーハ外周部における酸素濃度の分布特性δが0.5×1017atoms/cm3以下であることを満足し、引上げ速度の制御性が良好で、酸素濃度の増加やくねりも抑制され、さらに規定直径のウェーハに加工する際に廃棄される外周部の量が最小となるインゴットを得ることができる。
In the above formula 2, the limit value (allowable value) of the distribution characteristic δ of the oxygen concentration at the outer periphery of the wafer is 0.1 × 10 17 atoms / cm 3 , the limit value of the horizontal magnetic field strength is 2500 G, and a single crystal crystal when pulling up When the limit value of the rotation speed is set to 8 rpm and is substituted into the above equation 2, the diameter D of the silicon single crystal obtained by this is 330 mm. If a silicon single crystal is manufactured with this diameter D as a set value, the distribution characteristic δ of the oxygen concentration at the outer periphery of the wafer is satisfied to be 0.5 × 10 17 atoms / cm 3 or less, and the controllability of the pulling rate is high. It is possible to obtain an ingot that is good, suppresses an increase in oxygen concentration and bends, and further minimizes the amount of the outer peripheral portion discarded when processing into a wafer having a specified diameter.
上述した例においては、式2にウェーハ外周部における酸素濃度の分布特性δの限界値、水平磁場強度の限界値、及び引き上げる際の単結晶の結晶回転速度の限界値を代入し、これによりシリコン単結晶の直径Dを求めたが、これに代えて、式2にウェーハ外周部における酸素濃度の分布特性δの限界値、シリコン単結晶の直径の限界値、及び引き上げる際の単結晶の結晶回転速度の限界値を代入し、これにより水平磁場強度を求め、求められた水平磁場強度を設定してシリコン単結晶を製造してもよい。またこれに代えて、式2にウェーハ外周部における酸素濃度の分布特性δの限界値、シリコン単結晶の直径の限界値、及び水平磁場強度の限界値を代入し、これにより引き上げる際の単結晶の結晶回転速度を求め、求められた結晶回転速度を設定してシリコン単結晶を製造してもよい。
In the above-described example, the limit value of the distribution characteristic δ of the oxygen concentration at the outer periphery of the wafer, the limit value of the horizontal magnetic field strength, and the limit value of the crystal rotation speed of the single crystal at the time of pulling are substituted into Equation 2, thereby Although the diameter D of the single crystal was obtained, instead of this, the limit value of the oxygen concentration distribution characteristic δ at the outer periphery of the wafer, the limit value of the diameter of the silicon single crystal, and the crystal rotation of the single crystal at the time of pulling up A silicon single crystal may be manufactured by substituting the limit value of the velocity, thereby obtaining the horizontal magnetic field strength, and setting the obtained horizontal magnetic field strength. In place of this, the limit value of the distribution characteristic δ of the oxygen concentration at the outer periphery of the wafer, the limit value of the diameter of the silicon single crystal, and the limit value of the horizontal magnetic field strength are substituted into Equation 2, and the single crystal when pulling up by this is substituted. A single crystal of silicon may be manufactured by obtaining the crystal rotation speed of the first and setting the obtained crystal rotation speed.
1…シリコン単結晶の製造装置
11…第1チャンバ
12…第2チャンバ
13…ガス導入口
14…ガス排出口
21…石英製の坩堝
22…黒鉛製の坩堝
23…支持軸
24…駆動機構
25…ヒータ
26…保温筒
27…熱遮蔽部材
28…ブラケット
31…ワイヤ
32…引上げ機構
41…磁場発生装置
M…シリコン融液
C…シリコン単結晶
S…種結晶 DESCRIPTION OFSYMBOLS 1 ... Manufacturing apparatus of a silicon single crystal 11 ... 1st chamber 12 ... 2nd chamber 13 ... Gas inlet 14 ... Gas outlet 21 ... Quartz crucible 22 ... Graphite crucible 23 ... Support shaft 24 ... Drive mechanism 25 ... Heater 26 ... Insulating cylinder 27 ... Heat shielding member 28 ... Bracket 31 ... Wire 32 ... Pulling mechanism 41 ... Magnetic field generator M ... Silicon melt C ... Silicon single crystal S ... Seed crystal
11…第1チャンバ
12…第2チャンバ
13…ガス導入口
14…ガス排出口
21…石英製の坩堝
22…黒鉛製の坩堝
23…支持軸
24…駆動機構
25…ヒータ
26…保温筒
27…熱遮蔽部材
28…ブラケット
31…ワイヤ
32…引上げ機構
41…磁場発生装置
M…シリコン融液
C…シリコン単結晶
S…種結晶 DESCRIPTION OF
Claims (4)
- CZ法により引き上げる際の単結晶の直径と、融液に印加する水平磁場強度と、引き上げる際の単結晶の結晶回転速度と、ウェーハ外周部における酸素濃度の分布特性と、の相関関係を、所定の製造条件について予め求め、
前記ウェーハ外周部における酸素濃度の分布特性の限界値と、前記水平磁場強度の限界値と、前記引き上げる際の単結晶の結晶回転速度の限界値と、前記相関関係とから、引き上げる際の単結晶の最小の直径を求め、
当該求められた最小の直径を目標直径としてシリコン単結晶を前記所定の製造条件の下で製造するシリコン単結晶の製造方法。 The correlation between the diameter of the single crystal when pulled by the CZ method, the horizontal magnetic field strength applied to the melt, the crystal rotation speed of the single crystal when pulled, and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer are predetermined. Obtain in advance about the manufacturing conditions of
From the limit value of the oxygen concentration distribution characteristic at the outer periphery of the wafer, the limit value of the horizontal magnetic field strength, the limit value of the crystal rotation speed of the single crystal at the time of pulling up, and the correlation, the single crystal at the time of pulling up Find the smallest diameter of
A method for producing a silicon single crystal, wherein a silicon single crystal is produced under the predetermined production conditions using the determined minimum diameter as a target diameter. - CZ法により引き上げる際の単結晶の直径と、融液に印加する水平磁場強度と、引き上げる際の単結晶の結晶回転速度と、ウェーハ外周部における酸素濃度の分布特性と、の相関関係を、所定の製造条件について予め求め、
前記ウェーハ外周部における酸素濃度の分布特性の限界値と、前記引き上げる際の単結晶の直径の限界値と、前記引き上げる際の単結晶の結晶回転速度の限界値と、前記相関関係とから、印加する水平磁場強度を求め、
当該求められた水平磁場強度と前記所定の製造条件の下で単結晶を製造するシリコン単結晶の製造方法。 The correlation between the diameter of the single crystal when pulled by the CZ method, the horizontal magnetic field strength applied to the melt, the crystal rotation speed of the single crystal when pulled, and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer are predetermined. Obtain in advance about the manufacturing conditions of
Applied from the limit value of the distribution characteristic of the oxygen concentration in the outer periphery of the wafer, the limit value of the diameter of the single crystal when the pulling, the limit value of the crystal rotation speed of the single crystal when the pulling, and the correlation Find the horizontal magnetic field strength to
A method for producing a silicon single crystal, wherein a single crystal is produced under the obtained horizontal magnetic field strength and the predetermined production conditions. - CZ法により引き上げる際の単結晶の直径と、融液に印加する水平磁場強度と、引き上げる際の単結晶の結晶回転速度と、ウェーハ外周部における酸素濃度の分布特性と、の相関関係を、所定の製造条件について予め求め、
前記ウェーハ外周部における酸素濃度の分布特性の限界値と、前記引き上げる際の単結晶の直径の限界値と、前記水平磁場強度の限界値と、前記相関関係とから、前記引き上げる際の単結晶の結晶回転速度を求め、
当該求められた結晶回転速度と前記所定の製造条件の下で単結晶を製造するシリコン単結晶の製造方法。 The correlation between the diameter of the single crystal when pulled by the CZ method, the horizontal magnetic field strength applied to the melt, the crystal rotation speed of the single crystal when pulled, and the distribution characteristics of the oxygen concentration at the outer periphery of the wafer are predetermined. Obtain in advance about the manufacturing conditions of
From the limit value of the distribution characteristic of the oxygen concentration in the outer periphery of the wafer, the limit value of the diameter of the single crystal at the time of pulling up, the limit value of the horizontal magnetic field strength, and the correlation, the single crystal at the time of pulling up Find the crystal rotation speed,
A method for producing a silicon single crystal, comprising producing a single crystal under the determined crystal rotation speed and the predetermined production conditions. - 前記引き上げる際の単結晶の直径をD(mm)、水平磁場強度をG(ガウス)、前記引き上げる際の単結晶の結晶回転速度をV(rpm)、前記ウェーハ外周部における酸素濃度の分布特性をδ(1017atoms/cm3)、a,b,c,dを定数としたときに、δ=aD+bG+cV+dなる式により前記相関関係を定義し、前記所定の製造条件の下で予め前記定数a,b,c,dを求めておく請求項1~3のいずれか一項に記載のシリコン単結晶の製造方法。 The diameter of the single crystal at the time of pulling is D (mm), the horizontal magnetic field strength is G (Gauss), the crystal rotation speed of the single crystal at the time of pulling is V (rpm), and the distribution characteristics of oxygen concentration at the outer periphery of the wafer. When δ (10 17 atoms / cm 3 ), a, b, c, and d are constants, the correlation is defined by the following equation: δ = aD + bG + cV + d, and the constants a, The method for producing a silicon single crystal according to any one of claims 1 to 3, wherein b, c and d are obtained.
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JP2018002496A (en) | 2018-01-11 |
KR20180124975A (en) | 2018-11-21 |
JP6680108B2 (en) | 2020-04-15 |
KR102157389B1 (en) | 2020-09-17 |
TWI635199B (en) | 2018-09-11 |
TW201800626A (en) | 2018-01-01 |
CN109415843A (en) | 2019-03-01 |
DE112017003224B4 (en) | 2021-09-30 |
CN109415843B (en) | 2024-08-13 |
DE112017003224T5 (en) | 2019-03-21 |
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